CN104962769A - CBN (cubic boron nitride) polycrystalline sintered compact made by using nano-metal additives and method for manufacturing CBN polycrystalline sintered compact - Google Patents

CBN (cubic boron nitride) polycrystalline sintered compact made by using nano-metal additives and method for manufacturing CBN polycrystalline sintered compact Download PDF

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CN104962769A
CN104962769A CN201510347891.2A CN201510347891A CN104962769A CN 104962769 A CN104962769 A CN 104962769A CN 201510347891 A CN201510347891 A CN 201510347891A CN 104962769 A CN104962769 A CN 104962769A
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cbn
sintered compact
polycrystalline sintered
powder
auxiliary agent
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卢灿华
张涛
刘俊涛
窦明
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Zhongnan Diamond Co Ltd
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Zhongnan Diamond Co Ltd
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Abstract

The invention discloses CBN (cubic boron nitride) polycrystalline sintered compact made by using nano-metal additives and a method for manufacturing the CBN polycrystalline sintered compact, and belongs to the technical field of cubic boron nitride tool materials. The nano-metal additives comprise, by weight, 25-45% of TiN powder, 20-25% of TaC powder, 10-15% of AlB<2> powder, 15-20% of Co powder and 10-15% of Al powder. Formulas of the CBN polycrystalline sintered compact made by using the nano-metal additives are reasonably arranged and selected by the aid of nano-technologies, and accordingly technical bottleneck in the aspects of high toughness and high abrasion resistance of existing CBN polycrystalline sintered compact can be broken through. Compared with the existing CBN polycrystalline sintered compact, the CBN polycrystalline sintered compact made by using the nano-metal additives and the method have the advantages that the abrasion ratio can be increased and is 6000-7000 from the original 3500-5000; the micro-hardness HV (Vickers hardness) of working layers can be increased and is 5000-7000 from the original 2000-5000, and the bending strength can be increased and is 750-850MPa from the original 300-600MPa.

Description

A kind of CBN polycrystalline sintered compact using nano metal auxiliary agent to make and preparation method thereof
Technical field
The invention belongs to cubic boron nitride cutting tool Material Field, be specifically related to a kind of CBN polycrystalline sintered compact using nano metal auxiliary agent to make and preparation method thereof, it can be used as overall CBN glomerocryst cutting tool, can be used for cast iron, quenched steel, unmanageable half finish turning, finish turning and the millings such as high temperature steel alloy.
Background technology
CBN polycrystalline sintered compact is sintered at high temperature under high pressure by cubic boron nitride particle and the binding agent that forms by a certain percentage and forms, CBN cutter is as one of topmost superhard material, there is very high hardness, wear resistance, chemical stability, be suitable for the machining needs such as high speed cutting, hard turning, DRY CUTTING, in cutting cast iron, quenched steel, high temperature steel alloy and the Ferrious material such as Wimet, surface spraying, have unrivaled superiority.
At present, overall CBN glomerocryst cutting tool is very general in the application of western developed country, and the manufacture of CBN cutter and utilisation technology are quite ripe, and product is also towards variation, seriation development.The manufacturer of CBN cutter material can be provided abroad to mainly contain: the Sumitomo Electric Industries of the E6 company of D.I company of the U.S., Britain, the ILJIN company of Korea S, Japan.Their CBN product has developed more than 30 years, and has formed the tandem product being applicable to the various unlike material of processing, and because product is with strong points, steady quality is reliable, therefore monopolizes global most high-end market.
China has larger gap to overall CBN glomerocryst cutting tool and applied research thereof relative to western developed country, is specifically mainly manifested in the aspect such as cutting performance, cutter life.It is less, second-rate that domestic production manufactures polycrystal cubic boron nitride cutter product category, and overall strength is still weak.Domestic overall CBN cutter product is due to the restriction of recipe optimization, and Problems existing has: 1) wear resistance ratio is 3500 ~ 5000(is abroad about 5000 ~ 8000); 2) working lining microhardness HV is 2000 ~ 5000(is abroad about 4000 ~ 7000); 3) bending strength is 300 ~ 600 MPa(is abroad about 500 ~ 1000 MPa); This is different from the composition and engineering that each unit adopts relevant.
Summary of the invention
For overcoming prior art deficiency, the object of the invention is to provide a kind of CBN polycrystalline sintered compact using nano metal auxiliary agent to make and preparation method thereof, and it is CBN glomerocryst cutting tool as a whole, has high rate, high ductility feature.
For achieving the above object, the present invention adopts following technical scheme:
A kind of nano metal auxiliary agent, this auxiliary agent is made up of the raw material of following weight percent: TiN powder 25 ~ 45%, TaC powder 20 ~ 25%, AlB 2powder 10 ~ 15%, Co powder 15 ~ 20% and Al powder 10 ~ 15%.Each raw material of described auxiliary agent is good to use analytical pure, TiN, TaC and AlB 2particle diameter in 10 ~ 30nm, Co powder and Al powder footpath at 20 ~ 40nm time effect better, be more conducive to the toughness strengthening CBN polycrystalline sintered compact.
The CBN polycrystalline sintered compact using above-mentioned nano assistant to make, CBN polycrystalline sintered compact is made up of the raw material of following weight percent: CBN powder (particle diameter is good between 2 ~ 6 μm) 60 ~ 93% and nano metal auxiliary agent 7 ~ 40%.
The preparation method of the CBN polycrystalline sintered compact that above-mentioned use nano metal auxiliary agent is made, it comprises the steps:
1) purification and reduction treatment: CBN powder is first boiled 3 ~ 7min with the aqueous sodium hydroxide solution of 25 ~ 35wt%, deionized water wash is to neutral, 5 ~ 10min is boiled with nitration mixture (vitriol oil and concentrated nitric acid volume ratio are 1 ︰ 1), and with deionized water wash to neutral, and then boil 3 ~ 7min with chloroazotic acid (concentrated hydrochloric acid and concentrated nitric acid volume ratio are 3:1), and it is extremely neutral, for subsequent use with deionized water wash again; By nano metal auxiliary agent in hydrogen reducing furnace in 680 ~ 720 DEG C of reduction treatment 2 ~ 3h, for subsequent use;
2) batch mixing: take the CBN powder and nano metal auxiliary agent that processed in proportion, put into three-dimensional material mixer and carry out premix, three-dimensional material mixer is rotating speed: 95 ± 10 r/min, three-dimensional time: 10 ± 5 hours; Then by material mixed for three-dimensional, then planetary ball mill carries out batch mixing, and design parameter is as follows: material and sintered carbide ball (φ 6) weight ratio 1: 3 ~ 3.5; Be filled with liquid nitrogen from ball grinder end interface, liquid nitrogen is 1: 1 ~ 2 with the volume ratio of material and ball; Planetary ball mill parameter: revolution: 40 ± 5 r/min, rotation: 90 ± 5 r/min, Ball-milling Time: 15 ± 5 hours;
3) assembling of polycrystalline sintered compact and vacuum-treat: the CBN powder mixed is poured in graphite jig, then covers graphite flake and buckle metal molybdenum bowl cover; Polycrystalline sintered compact assembly is placed in vacuum apparatus, under vacuum state, passes into appropriate hydrogen, be not more than 3 × 10 -5in 680 ~ 780 DEG C of insulations 3 ~ 4 hours under the vacuum condition of Pa;
4) High Temperature High Pressure sintering: the polycrystalline sintered compact assembly of vacuum-treat is placed in synthesis assembly block in, with six-plane piercer temperature be 1470 ± 20 DEG C, pressure be the condition of 5.5 ~ 6GPa under synthesis 20 ~ 30min.
Except as otherwise noted, the vitriol oil in the present invention all refers to that density is 1.84gcm -the sulfuric acid of 3, concentrated nitric acid all refers to that density is 1. 4 gcm -the nitric acid of 3, concentrated hydrochloric acid all refers to that density is 1.179 gcm -the hydrochloric acid of 3.
Nano metal auxiliary agent CBN polycrystalline sintered compact of the present invention by have employed the nano materials such as TiN, TaC, Al and Co in formula, its dominant mechanism is: TiN and TaC has high rigidity, high-melting-point and high heat conductivity, and aluminium can react with cubic boron nitride and generates AlN, the carrying out of acceleration of sintering in sintering process.Simultaneously, AlN can suppress CBN to the reversal of HBN, for the polycrystalline cubic boron nitride content and the density important role that improve composite sheet, cobalt mainly plays the cleaning action that " deoxidation is degassed " is carried out on cubic boron nitride surface, activation cubic boron nitride microparticle, promote the performance of directly Cheng Jian, raising CBN glomerocryst composite sheet between cubic boron nitride particle.
In this preparation method, according to the size-grade distribution feature of cubic boron nitride, determine optimum vacuum treatment process scope, cubic boron nitride particle surface is obtained fully " purification, activation ", and the impurity such as the oxygen of a large amount of absorption are desorbed and pump outside cbn layer; According to melts combine agent material reduction characteristic, passed into appropriate hydrogen under vacuum conditions, the reductive action due to hydrogen makes bonding agent surfactivity increase, and is easy to make them chemical action occur and improve bonding strength between cubic boron nitride particle.
In this preparation method, synthesis assembly block structure used have employed pyrophyllite ring and rhombspar bushing pipe as outer pressure transmission thermal insulation medium; Carbon pipe, salt pipe and salt sheet are as interior transmission medium, be evenly distributed to make the temperature, pressure in synthesis chamber, ensure that residing for synthesised polycrystalline sintered compact, high pressure-temperature field is more stable: (1) conducting steel ring adopts large diameter thin wall structure, heart portion filling rhombspar core and outer race pyrophyllite ring, be incubated to realize two ends and avoid burning hammer.(2) special-shaped electrical conductor adopts the material that resistivity is higher, by changing its shape and adjust size, reduces synthetic cavity thermograde.(3) in carbon pipe salt adding pipe, salt sheet as interior transmission medium because salt it had not only had mobility but also had had the feature of expansion at high temperature under high pressure, can effective transmission of pressure, reduce the pressure gradient of large cavity.(4) sintered compact adopts two high temperature resistant molybdenum cups to close cubic boron nitride powder, well can play shielding effect, can not be subject to the pollution of foreign matter when cubic boron nitride is sintered.
The CBN polycrystalline sintered compact that the present invention uses nano metal auxiliary agent to make, in formula, utilizes nanotechnology reasonable arrangement and selects to fill a prescription, and breaches the technical bottleneck of CBN polycrystalline sintered compact high tenacity and high-wearing feature.Compared with existing CBN polycrystalline sintered compact: wear resistance ratio brings up to 6000 ~ 7000 by 3500 ~ 5000; Working lining microhardness HV brings up to 5000 ~ 7000 by 2000 ~ 5000, and bending strength brings up to 750 ~ 850MPa by 300 ~ 600 MPa.Illustrate that nano material bonding agent has at high temperature under high pressure and sinter promoter action preferably, contribute to sintering and improve the volume ratio of CBN glomerocryst, be conducive to forming tough sintered compact, add the toughness of CBN polycrystalline sintered compact, increase the service life.
Embodiment
Below by way of preferred embodiment, present invention process is described in further detail, but protection scope of the present invention is not limited thereto.
embodiment 1
A kind of CBN polycrystalline sintered compact using nano metal auxiliary agent to make, be made up of the raw material of following weight percent: CBN powder (2 ~ 6 μm) 60% and nano metal auxiliary agent 40%, described nano metal auxiliary agent is made up of the raw material of following weight percent: analytical pure TiN powder (8 ~ 12nm) 45%, analytical pure TaC powder (8 ~ 12nm) 20%, analytical pure AlB 2powder (8 ~ 12nm) 10%, analytical pure Co powder (22 ~ 36nm) 15% and analytical pure Al powder (22 ~ 36nm) 10%.
The preparation method of above-mentioned CBN polycrystalline sintered compact, it comprises the steps:
1) purification and reduction treatment: CBN powder is first boiled 7min with the aqueous sodium hydroxide solution of 35wt%, deionized water wash is to neutral, 10min is boiled with nitration mixture (vitriol oil and concentrated nitric acid volume ratio are 1 ︰ 1), and with deionized water wash to neutral, and then boil 7min with chloroazotic acid (concentrated hydrochloric acid and concentrated nitric acid volume ratio are 3 ︰ 1), and it is extremely neutral, for subsequent use with deionized water wash again; By nano metal auxiliary agent in hydrogen reducing furnace in 720 DEG C of reduction treatment 3h, for subsequent use;
2) batch mixing: take the CBN powder and nano metal auxiliary agent that processed in proportion, put into three-dimensional material mixer and carry out premix, three-dimensional material mixer rotating speed is: 105 r/min, three-dimensional time: 15 hours; Then by material mixed for three-dimensional, then planetary ball mill carries out batch mixing, and design parameter is as follows: material and sintered carbide ball (φ 6) weight ratio 1 ︰ 3.5; Be filled with liquid nitrogen from ball grinder end interface, liquid nitrogen is 1 ︰ 2 with the volume ratio of material and ball; Planetary ball mill parameter: revolution: 45 r/min, rotation: 95 r/min, Ball-milling Time: 20 hours;
3) assembling of polycrystalline sintered compact and vacuum-treat: the CBN powder mixed is poured in graphite jig, then covers graphite flake and buckle metal molybdenum bowl cover; Polycrystalline sintered compact assembly is placed in vacuum apparatus, passes into appropriate hydrogen (often burn a slice CBN polycrystalline sintered compact and need 1L hydrogen, be lower same) under vacuum state, be not more than 3 × 10 -5in 780 DEG C of insulations 4 hours under the vacuum condition of Pa;
4) High Temperature High Pressure sintering: the polycrystalline sintered compact assembly of vacuum-treat is placed in synthesis assembly block, with six-plane piercer temperature be 1490 DEG C, pressure synthesizes 30min under being the condition of 6GPa.
The key technical indexes of obtained CBN polycrystalline sintered compact: 1) wear resistance ratio is 6000,2) working lining microhardness HV is 5500,3) bending strength is 800 MPa.
embodiment 2
A kind of nano metal auxiliary agent CBN polycrystalline sintered compact, be made up of the raw material of following weight percent: CBN powder (2 ~ 6 μm) 93% and nano metal auxiliary agent 7%, described nano metal auxiliary agent is made up of the raw material of following weight percent: analytical pure TiN powder (8 ~ 12nm) 25%, analytical pure TaC powder (8 ~ 12nm) 25%, analytical pure AlB 2powder (8 ~ 12nm) 15%, analytical pure Co powder (22 ~ 36nm) 20% and analytical pure Al powder (22 ~ 36nm) 15%.
The preparation method of above-mentioned CBN polycrystalline sintered compact, it comprises the steps:
1) purification and reduction treatment: CBN powder is first boiled 3min with the aqueous sodium hydroxide solution of 25%, deionized water wash is to neutral, 5min is boiled with nitration mixture (vitriol oil and concentrated nitric acid volume ratio are 1 ︰ 1), and with deionized water wash to neutral, and then boil 3min with chloroazotic acid (concentrated hydrochloric acid and concentrated nitric acid volume ratio are 3 ︰ 1), and it is extremely neutral, for subsequent use with deionized water wash again; By nano metal auxiliary agent in hydrogen reducing furnace in 680 DEG C of reduction treatment 2h, for subsequent use;
2) batch mixing: take the CBN powder and nano metal auxiliary agent that processed in proportion, put into three-dimensional material mixer and carry out premix, three-dimensional material mixer is rotating speed: 85 r/min, three-dimensional time: 5 hours; Then by material mixed for three-dimensional, then planetary ball mill carries out batch mixing, and design parameter is as follows: material and sintered carbide ball (φ 6) weight ratio 1 ︰ 3; Be filled with liquid nitrogen from ball grinder end interface, liquid nitrogen is 1 ︰ 1 with the volume ratio of material and ball; Planetary ball mill parameter: revolution: 35 r/min, rotation: 85 r/min, Ball-milling Time: 10 hours;
3) assembling of polycrystalline sintered compact and vacuum-treat: the CBN powder mixed is poured in graphite jig, then covers graphite flake and buckle metal molybdenum bowl cover; Polycrystalline sintered compact assembly is placed in vacuum apparatus, under vacuum state, passes into appropriate hydrogen, be not more than 3 × 10 -5in 680 DEG C of insulations 3 hours under the vacuum condition of Pa;
4) High Temperature High Pressure sintering: the polycrystalline sintered compact assembly of vacuum-treat is placed in synthesis assembly block, with six-plane piercer temperature be 1450 DEG C, pressure synthesizes 20min under being the condition of 5.5GPa.
The key technical indexes of obtained CBN polycrystalline sintered compact: 1) wear resistance ratio is 6700,2) working lining microhardness HV is 6000,3) bending strength is 700 MPa.
embodiment 3
A kind of nano metal auxiliary agent CBN polycrystalline sintered compact, be made up of the raw material of following weight percent: CBN powder (2 ~ 6 μm) 85% and nano metal auxiliary agent 15%, described nano metal auxiliary agent is made up of the raw material of following weight percent: analytical pure TiN powder (8 ~ 12nm) 35%, analytical pure powder TaC(8 ~ 12nm) 22.5%, analytical pure AlB 2powder (8 ~ 12nm) 12.5%, analytical pure Co powder (22 ~ 36nm) 17.5% and analytical pure Al powder (22 ~ 36nm) 12.5%.
The preparation method of above-mentioned CBN polycrystalline sintered compact, it comprises the steps:
1) purification and reduction treatment: CBN powder is first boiled 5min with the aqueous sodium hydroxide solution of 30wt%, deionized water wash is to neutral, 7min is boiled with nitration mixture (vitriol oil and concentrated nitric acid volume ratio are 1 ︰ 1), and with deionized water wash to neutral, and then boil 5min with chloroazotic acid (concentrated hydrochloric acid and concentrated nitric acid volume ratio are 3 ︰ 1), and it is extremely neutral, for subsequent use with deionized water wash again; By nano metal auxiliary agent in hydrogen reducing furnace in 700 DEG C of reduction treatment 2.5h, for subsequent use;
2) batch mixing: take the CBN powder and nano metal auxiliary agent that processed in proportion, put into three-dimensional material mixer and carry out premix, three-dimensional material mixer is rotating speed: 95r/min, three-dimensional time: 10 hours; Then by material mixed for three-dimensional, then planetary ball mill carries out batch mixing, and design parameter is as follows: material and sintered carbide ball (φ 6) weight ratio 1 ︰ 3.1; Be filled with liquid nitrogen from ball grinder end interface, liquid nitrogen is 1 ︰ 1.5 with the volume ratio of material and ball; Planetary ball mill parameter: revolution: 40 r/min, rotation: 90 r/min, Ball-milling Time: 15 hours;
3) assembling of polycrystalline sintered compact and vacuum-treat: the CBN powder mixed is poured in graphite jig, then covers graphite flake and buckle metal molybdenum bowl cover; Polycrystalline sintered compact assembly is placed in vacuum apparatus, under vacuum state, passes into appropriate hydrogen, be not more than 3 × 10 -5in 730 DEG C of insulations 3.5 hours under the vacuum condition of Pa;
4) High Temperature High Pressure sintering: the polycrystalline sintered compact assembly of vacuum-treat is placed in synthesis assembly block, with six-plane piercer temperature be 1470 DEG C, pressure synthesizes 28min under being the condition of 5.6GPa.
The key technical indexes of obtained CBN polycrystalline sintered compact: 1) wear resistance ratio is 7500,2) working lining microhardness HV is 6800,3) bending strength is 850MPa.

Claims (4)

1. a nano metal auxiliary agent, is characterized in that, this auxiliary agent is made up of the raw material of following weight percent: TiN powder 25 ~ 45%, TaC powder 20 ~ 25%, AlB 2powder 10 ~ 15%, Co powder 15 ~ 20% and Al powder 10 ~ 15%.
2. use the CBN polycrystalline sintered compact that nano metal auxiliary agent described in claim 1 is made, it is characterized in that, this CBN polycrystalline sintered compact is made up of the raw material of following weight percent: CBN powder 60 ~ 93% and nano metal auxiliary agent 7 ~ 40%.
3. the preparation method of the CBN polycrystalline sintered compact using nano metal auxiliary agent to make described in claim 2, is characterized in that, comprise the steps:
1) purification and reduction treatment: CBN powder is first boiled 3 ~ 7min with the aqueous sodium hydroxide solution of 25 ~ 35wt%, deionized water wash is to neutral, 5 ~ 10min is boiled with nitration mixture, and with deionized water wash to neutral, and then boil 3 ~ 7min with chloroazotic acid, and it is extremely neutral, for subsequent use with deionized water wash again; By nano metal auxiliary agent in hydrogen reducing furnace in 680 ~ 720 DEG C of reduction treatment 2 ~ 3h, for subsequent use;
2) batch mixing: take the CBN powder and nano metal auxiliary agent that processed in proportion, put into three-dimensional material mixer and carry out premix, three-dimensional material mixer rotating speed is: 95 ± 10 r/min, the time: 10 ± 5 hours; Then by material mixed for three-dimensional material mixer, then carry out batch mixing with planetary ball mill, design parameter is as follows: material and sintered carbide ball weight ratio 1: 3 ~ 3.5; Be filled with liquid nitrogen from ball grinder end interface, liquid nitrogen is 1: 1 ~ 2 with the volume ratio of material and ball; Planetary ball mill parameter: revolution: 40 ± 5 r/min, rotation: 90 ± 5 r/min, Ball-milling Time: 15 ± 5 hours;
3) assembling of polycrystalline sintered compact and vacuum-treat: the CBN powder mixed is poured in graphite jig, then covers graphite flake and buckle metal molybdenum bowl cover; Polycrystalline sintered compact assembly is placed in vacuum apparatus, is not more than 3 × 10 -5in 680 ~ 780 DEG C of insulations 3 ~ 4 hours under the vacuum condition of Pa;
4) High Temperature High Pressure sintering: the polycrystalline sintered compact assembly of vacuum-treat is placed in synthesis assembly block in, with six-plane piercer temperature be 1470 ± 20 DEG C, pressure be the condition of 5.5 ~ 6GPa under synthesis 20 ~ 30min.
4. the preparation method of CBN polycrystalline sintered compact described in claim 3, is characterized in that, the nitration mixture described in step 1) is volume ratio is 1 ︰ 1 vitriol oil and concentrated nitric acid.
CN201510347891.2A 2015-06-23 2015-06-23 CBN (cubic boron nitride) polycrystalline sintered compact made by using nano-metal additives and method for manufacturing CBN polycrystalline sintered compact Pending CN104962769A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
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Application publication date: 20151007